CN113644149B - 提高CdZnTe探测器性能的CdZnTe/GaAs外延膜及制备方法 - Google Patents
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Abstract
本发明涉及一种提高CdZnTe探测器性能的CdZnTe/GaAs外延膜及制备方法，基于P型GaAs衬底上生长CdZnTe厚膜并在Te2气氛中进行等温退火。将其制备成Au/CdZnTe/p‑GaAs/Au探测器，与退火之前相比，CdZnTe外延膜的电阻率明显提高，探测器对241Am@5.49MeVα粒子响应更加灵敏，能量分辨率提高，并且在退火之后出现了对241Am@59.5KeVγ射线的响应。本发明提供的改性方法包括衬底的预处理、CdZnTe外延膜的生长过程、CdZnTe外延膜的退火过程及辐射探测器的制备。
Description
技术领域
本发明属于CdZnTe探测器技术领域，涉及一种提高CdZnTe探测器性能的CdZnTe/GaAs外延膜及制备方法，特别涉及碲锌镉半导体外延薄膜材料探测性能的提高方法。
背景技术
Cd1-xZnxTe(简称为CdZnTe或CZT)是一种具有优异光电性能的II-VI族化合物半导体，其具有较高的原子序数，较大的禁带宽度，较高的本征μτ值，较低的电子-空穴电离能等优点，被认为是理想的室温X射线和γ射线探测器材料。目前，用CZT单晶体材料制作的室温辐射探测器已经被广泛应用于核医学、工业无损检测、航空航天及天体物理等领域。
传统熔体法生长会存在的效率低、晶锭利用率低及废料不能回收利用等问题，而近空间升华法很好地解决了这一点。CSS法生长薄膜提高了生长效率，但由于外延异质结中薄膜与衬底之间存在失配，外延膜中不可避免地存在着大量的结构缺陷和电杂质，在能带中引入陷阱能级。这些能级对载流子产生复合、俘获和散射等作用过程，从而影响载流子寿命、迁移率等运输特性，最终影响CZT探测器的能量分辨率、电荷收集率等探测性能。对于室温核辐射探测器，其高性能的关键在于高质量的CZT薄膜，要求具有较高的电阻(>1010Ω·cm)、较大的载流子迁移率寿命积。要获得高质量的CZT薄膜，一方面可以探索合适的生长工艺，控制在生长过程中便可获得缺陷较少的外延膜；另一方面可以对外延膜进行退火改性处理，进一步降低缺陷。
CSS法生长的CZT薄膜的主要缺陷是位错与点缺陷，位错包括界面位错与穿透位错，其破坏了晶格完整性，降低了探测器的能量分辨率和电阻率；而点缺陷的存在也会对探测器的电阻率产生很大影响，本发明将基于CSS法生长CZT薄膜，对其进行Te2气氛退火改性，调整薄膜中的位错密度和本征点缺陷浓度，以达到改善薄膜光电性能的目的。
CSS法生长的CdZnTe外延膜由于晶格失配不可避免地存在着点缺陷和位错，其破坏了晶格完整性并降低了探测器的能量分辨率和电阻率。
发明内容
要解决的技术问题
为了避免现有技术的不足之处，本发明提出一种提高CdZnTe探测器性能的CdZnTe/GaAs外延膜及制备方法，通过首先在GaAs衬底上生长CdZnTe外延膜，然后在Te2气氛中等温退火，调控外延膜中的缺陷，最终制备成Au/CdZnTe/p-GaAs/Au探测器并达到提高探测器探测性能的目的。
技术方案
一种提高CdZnTe探测器性能的CdZnTe/GaAs外延膜，其特征在于：在GaAs衬底上生长CdZnTe外延膜，然后在Te2气氛中等温退火，得到CdZnTe/GaAs外延膜。
一种制备所述CdZnTe/GaAs外延膜的方法，其特征在于步骤如下：
步骤1、衬底的预处理：将GaAs衬底在室温下，分别在丙酮、无水乙醇和去离子水中超声清洗以去除表面的杂质及有机物；清洗完成后，将衬底在H2SO4:H2O2:H2O＝4:1:1溶液中刻蚀20s，刻蚀完成后用去离子水冲洗，最后用氮气吹干放入近空间升华炉的上加热台；
步骤2、CdZnTe多晶源的预处理：将多晶源用砂纸打磨源表面的氧化层，之后在室温下分别在丙酮、无水乙醇和去离子水中超声清洗以去除表面的杂质及有机物；最后用氮气吹干放入近空间升华炉的下加热台；
步骤3、生长程序的设置：近空间升华炉的上下加热台分别控制衬底和多晶源的温度，外延膜的生长采用两步法，即上加热台的温度首先升温至833K下保温0.5h，再降到730K保温3.5h，下加热台的温度始终保持在983K，生长时间为4h；
步骤4、CdZnTe外延膜的生长：打开近空间升华炉，将经过预处理的多晶源和衬底放入升华炉，开启机械泵和通气阀，待腔体真空度低于5Pa时分子泵自动接入，将腔内真空度抽至0.05Pa，运行步骤3的生长程序并打开水冷，待程序运行完成且炉内冷却至室温，依次关闭通气阀、分子泵及水冷，取出CdZnTe/GaAs外延膜；
步骤5、CdZnTe外延膜的退火：打开近空间升华炉，将退火源和CdZnTe/GaAs外延膜放入升华炉，开启机械泵和通气阀，待腔体真空度低于10Pa时运行退火程序；退火为恒温退火，退火源为粉状Te单质；上下加热台分别控制CdZnTe/GaAs外延膜与退火源的温度；打开水冷并关闭通气阀和机械泵，待程序运行完成且炉内冷却至室温，关闭水冷，制备完成CdZnTe/GaAs外延膜。
所述超声清洗为20～25分钟
所述GaAs衬底的面积小于多晶源的面积。
所述粉状Te单质纯度为7N。
一种采用所述CdZnTe/GaAs外延膜的CdZnTe探测器，其特征在于：在CdZnTe/GaAs的外延膜和衬底表面上，结合不超过100nm的金电极层，形成Au/CdZnTe/p-GaAs/Au探测器。
一种采用所述CdZnTe/GaAs外延膜的CdZnTe探测器，其特征在于：采用真空蒸镀法，将CdZnTe/GaAs外延膜放入蒸镀机，将真空度抽至0.005Pa，分别在外延膜和衬底表面蒸镀80nm的金电极层，形成Au/CdZnTe/p-GaAs/Au探测器。
一种所述CdZnTe探测器的应用方法，其特征在于：所述Au/CdZnTe/p-GaAs/Au探测器用于对241Am@59.5KeVγ射线的响应。
有益效果
本发明提出的一种提高CdZnTe探测器性能的CdZnTe/GaAs外延膜及制备方法，基于P型GaAs衬底上生长CdZnTe厚膜并在Te2气氛中进行等温退火。将其制备成Au/CdZnTe/p-GaAs/Au探测器，与退火之前相比，CdZnTe外延膜的电阻率明显提高，探测器对241Am@5.49MeVα粒子响应更加灵敏，能量分辨率提高，并且在退火之后出现了对241Am@59.5KeVγ射线的响应。本发明提供的改性方法包括衬底的预处理、CdZnTe外延膜的生长过程、CdZnTe外延膜的退火过程及辐射探测器的制备。
本明将退火后的CdZnTe外延膜制备成Au/CdZnTe/p-GaAs/Au探测器，与退火之前相比，CdZnTe外延膜的电阻率明显提高，探测器对241Am@5.49MeVα粒子响应更加灵敏，能量分辨率提高，并且在退火之后出现了对241Am@59.5KeVγ射线的响应。
附图说明
图1为本发明实施例一CdZnTe外延膜退火后和对比例生长态CdZnTe外延膜的EPD扫描图。
图2为本发明实施例一CdZnTe外延膜退火后制成Au/CdZnTe/p-GaAs/Au探测器和对比例生长态CdZnTe外延膜制成Au/CdZnTe/p-GaAs/Au探测器的I-V曲线图。
图3为本发明实施例一CdZnTe外延膜退火后制成Au/CdZnTe/p-GaAs/Au探测器和生长态CdZnTe外延膜制成Au/CdZnTe/p-GaAs/Au探测器在241Am@5.49MeVα粒子作用下通过Hecht方程拟合的电子迁移率寿命积。
图4为本发明实施例一CdZnTe外延膜退火后制成Au/CdZnTe/p-GaAs/Au探测器测得241Am@59.5KeVγ射线的全能峰。
具体实施方式
现结合实施例、附图对本发明作进一步描述：
实施例一
在本实施例中，一种提高CdZnTe外延膜探测器性能方法，其特征在于：首先在GaAs衬底上生长CdZnTe外延膜，然后在Te2气氛中等温退火，最终制备成Au/CdZnTe/p-GaAs/Au探测器。CdZnTe外延膜的厚度为280um，GaAs衬底的厚度为550um。
在本实施中，本实施例具有Au/CdZnTe/p-GaAs/Au探测器的制备方法，其步骤如下：
衬底的预处理：将厚度为550um的GaAs衬底切割成12×12mm2大小的方块，室温下分别在丙酮、无水乙醇和去离子水中超声清洗20到25分钟以去除表面的杂质及有机物；清洗完成后，将衬底在H2SO4:H2O2:H2O＝4:1:1溶液中刻蚀20s，刻蚀完成后用去离子水冲洗，最后用氮气吹干放入近空间升华炉备用。
CdZnTe多晶源的预处理：将厚度为2mm的多晶源切割成15×15mm2大小的方块，用1000目的砂纸打磨源表面的氧化层，之后在室温下分别在丙酮、无水乙醇和去离子水中超声清洗20到25分钟以去除表面的杂质及有机物；最后用氮气吹干放入近空间升华炉备用。
生长程序的设置：近空间升华炉的上下加热台分别控制衬底和多晶源的温度，外延膜的生长采用两步法，即上加热台的温度首先升温至833K下保温0.5h，再降到730K保温3.5h，下加热台的温度始终保持在983K，生长时间为4h。
CdZnTe外延膜的生长过程：打开近空间升华炉，将经过预处理的多晶源和衬底放入升华炉，开启机械泵和通气阀，待腔体真空度低于5Pa时分子泵自动接入，将腔内真空度抽至0.05Pa，运行生长程序并打开水冷，待程序运行完成且炉内冷却至室温，依次关闭通气阀、分子泵及水冷，取出CdZnTe/GaAs外延膜，CdZnTe外延膜的厚度为280um。
CdZnTe外延膜的退火过程：打开近空间升华炉，将退火源和外延膜放入升华炉，开启机械泵和通气阀，待腔体真空度低于10Pa时运行退火程序，退火为恒温退火，退火源为粉状Te单质，纯度为7N；上下加热台分别控制外延膜与退火源的温度，上下加热台的温度都加热至623K并保温10h。打开水冷并关闭通气阀和机械泵，待程序运行完成且炉内冷却至室温，关闭水冷，取出CdZnTe/GaAs外延膜。
一种辐射探测器，在CdZnTe/GaAs的外延膜和衬底表面上，结合不超过100nm的金电极层，形成Au/CdZnTe/p-GaAs/Au探测器。
一种辐射探测器的制备方法，制备步骤如下：采用真空蒸镀法，将CdZnTe/GaAs外延膜放入蒸镀机，将真空度抽至0.005Pa，分别在外延膜和衬底表面蒸镀80nm的金电极层，形成Au/CdZnTe/p-GaAs/Au探测器。
一种辐射探测器的应用，将Au/CdZnTe/p-GaAs/Au探测器能对241Am@59.5KeVγ射线的响应。
本发明与现有技术相比较，具有如下显而易见的实质性特点和优点：
本明将退火后的CdZnTe外延膜制备成Au/CdZnTe/p-GaAs/Au探测器，与退火之前相比，CdZnTe外延膜的电阻率明显提高，探测器对241Am@5.49MeVα粒子响应更加灵敏，能量分辨率提高，并且在退火之后出现了对241Am@59.5KeVγ射线的响应。
对比例：
在本对比中，一种Au/CdZnTe/p-GaAs/Au探测器，首先在GaAs衬底上生长CdZnTe外延膜，然后再外延膜和衬底表面蒸镀不超过100nm的金电极层，最终制备成Au/CdZnTe/p-GaAs/Au探测器。CdZnTe外延膜的厚度为270um，GaAs衬底的厚度为550um。
结合实施例和对比例，有关本实施例通过在Te2气氛下退火处理的CdZnTe外延膜制备成Au/CdZnTe/p-GaAs/Au探测器和对比例直接用生长态的CdZnTe外延膜制备成的Au/CdZnTe/p-GaAs/Au探测器，采用实验仪器测试所得附图的解释说明如下：
图1的(a)和(b)分别本发明实施例一CdZnTe外延膜退火后和对比例生长态CdZnTe外延膜的EPD扫描图，退火后外延膜和生长态外延膜的位错腐蚀坑密度分别为2.29×105和1.56×105cm-2，位错密度明显下降。
图2为本发明实施例一CdZnTe外延膜退火后制成Au/CdZnTe/p-GaAs/Au探测器和对比例生长态CdZnTe外延膜制成Au/CdZnTe/p-GaAs/Au探测器的I-V曲线图。退火后和生长态外延膜制成的探测器的电阻率分别为4.38×109Ω·cm和5.47×108Ω·cm，退火处理可以明显提高探测器的电阻率。
图3为本发明实施例一CdZnTe外延膜退火后制成Au/CdZnTe/p-GaAs/Au探测器和生长态CdZnTe外延膜制成Au/CdZnTe/p-GaAs/Au探测器在241Am@5.49MeVα粒子作用下通过Hecht方程拟合的电子迁移率寿命积。退火后和生长态外延膜制成的探测器的电子迁移率寿命积分别为9.30×10-4cm2·V-1和5.27×10-4cm2·V-1，退火处理可以明显提高探测器的电子迁移率寿命积。
图4为本发明实施例一CdZnTe外延膜退火后制成Au/CdZnTe/p-GaAs/Au探测器测得241Am@59.5KeVγ射线的全能峰，而生长态外延膜制成的Au/CdZnTe/p-GaAs/Au探测器无法对241Am@59.5KeVγ射线产生响应。
本实施例可以使CdZnTe外延膜制成的探测器电阻率明显提高，对241Am@5.49MeVα粒子响应更加灵敏，能量分辨率提高，并且在对241Am@59.5KeVγ射线产生响应。
实施例二
本实施例与实施例一基本相同，特别之处在于：
在本实施例中，对于CdZnTe外延膜的退火过程，其退火过程如下：
退火过程：打开近空间升华炉，将退火源和外延膜放入升华炉，开启机械泵和通气阀，待腔体真空度低于10Pa时运行退火程序，退火为恒温退火，退火源为粉状Te单质，纯度为7N；上下加热台分别控制外延膜与退火源的温度，上下加热台的温度都加热至623K并保温5h。打开水冷并关闭通气阀和机械泵，待程序运行完成且炉内冷却至室温，关闭水冷，取出CdZnTe/GaAs外延膜。
本实施例可使CdZnTe外延膜制成的探测器电阻率稍有提高，对241Am@5.49MeVα粒子响应变灵敏，能量分辨率稍有提高，但未对241Am@59.5KeVγ射线产生响应。
实施例三
本实施例与实施例一基本相同，特别之处在于：
在本实施例中，对于CdZnTe外延膜的退火过程，其退火过程如下：
退火过程：打开近空间升华炉，将退火源和外延膜放入升华炉，开启机械泵和通气阀，待腔体真空度低于10Pa时运行退火程序，退火为恒温退火，退火源为粉状Te单质，纯度为7N；上下加热台分别控制外延膜与退火源的温度，上下加热台的温度都加热至673K并保温10h。打开水冷并关闭通气阀和机械泵，待程序运行完成且炉内冷却至室温，关闭水冷，取出CdZnTe/GaAs外延膜。
本实施例可使CdZnTe外延膜制成的探测器电阻率稍有提高，对241Am@5.49MeVα粒子响应变灵敏，能量分辨率稍有提高，但未对241Am@59.5KeVγ射线产生响应。
综上所述，本发明上述实施例提供了一种提高CdZnTe探测器外延膜性能的方法，包括在GaAs衬底上生长CdZnTe外延膜，然后在Te2气氛中不同条件下等温退火，最终制备成Au/CdZnTe/p-GaAs/Au探测器3个步骤。本发明上述实施例可以使CdZnTe外延膜制成的探测器电阻率明显提高，对241Am@5.49MeVα粒子响应更加灵敏，能量分辨率提高，并且在对241Am@59.5KeVγ射线产生响应。
上面对本发明实施例结合附图进行了说明，但本发明不限于上述实施例，还可以根据本发明做出多种变化，凡依据本发明技术方案的精神实质和原理下做的改变、修饰、替代或简化，均应为等效的置换方式，只要符合本发明的发明目的，不背离本发明具有对CdZnTe探测器外延膜在Te2下退火的技术原理，都属于本发明的保护范围。
Claims (8)
1.一种提高CdZnTe探测器性能的CdZnTe/GaAs外延膜，其特征在于：在GaAs衬底上生长CdZnTe外延膜，然后在Te2气氛中等温退火，得到CdZnTe/GaAs外延膜；
所述提高CdZnTe探测器性能的CdZnTe/GaAs外延膜是按照以下步骤制得：
步骤1、衬底的预处理：将GaAs衬底在室温下，分别在丙酮、无水乙醇和去离子水中超声清洗以去除表面的杂质及有机物；清洗完成后，将衬底在H2SO4:H2O2:H2O＝4:1:1溶液中刻蚀20s，刻蚀完成后用去离子水冲洗，最后用氮气吹干放入近空间升华炉的上加热台；
步骤2、CdZnTe多晶源的预处理：将多晶源用砂纸打磨源表面的氧化层，之后在室温下分别在丙酮、无水乙醇和去离子水中超声清洗以去除表面的杂质及有机物；最后用氮气吹干放入近空间升华炉的下加热台；
步骤3、生长程序的设置：近空间升华炉的上下加热台分别控制衬底和多晶源的温度，外延膜的生长采用两步法，即上加热台的温度首先升温至833K下保温0.5h，再降到730K保温3.5h，下加热台的温度始终保持在983K，生长时间为4h；
步骤4、CdZnTe外延膜的生长：打开近空间升华炉，将经过预处理的多晶源和衬底放入升华炉，开启机械泵和通气阀，待腔体真空度低于5Pa时分子泵自动接入，将腔内真空度抽至0.05Pa，运行步骤3的生长程序并打开水冷，待程序运行完成且炉内冷却至室温，依次关闭通气阀、分子泵及水冷，取出CdZnTe/GaAs外延膜；
步骤5、CdZnTe外延膜的退火：打开近空间升华炉，将退火源和CdZnTe/GaAs外延膜放入升华炉，开启机械泵和通气阀，待腔体真空度低于10Pa时运行退火程序；退火为恒温退火，退火源为粉状Te单质；上下加热台分别控制CdZnTe/GaAs外延膜与退火源的温度；打开水冷并关闭通气阀和机械泵，待程序运行完成且炉内冷却至室温，关闭水冷，制备完成CdZnTe/GaAs外延膜。
2.一种制备权利要求1所述CdZnTe/GaAs外延膜的方法，其特征在于步骤如下：
步骤1、衬底的预处理：将GaAs衬底在室温下，分别在丙酮、无水乙醇和去离子水中超声清洗以去除表面的杂质及有机物；清洗完成后，将衬底在H2SO4:H2O2:H2O＝4:1:1溶液中刻蚀20s，刻蚀完成后用去离子水冲洗，最后用氮气吹干放入近空间升华炉的上加热台；
步骤2、CdZnTe多晶源的预处理：将多晶源用砂纸打磨源表面的氧化层，之后在室温下分别在丙酮、无水乙醇和去离子水中超声清洗以去除表面的杂质及有机物；最后用氮气吹干放入近空间升华炉的下加热台；
步骤3、生长程序的设置：近空间升华炉的上下加热台分别控制衬底和多晶源的温度，外延膜的生长采用两步法，即上加热台的温度首先升温至833K下保温0.5h，再降到730K保温3.5h，下加热台的温度始终保持在983K，生长时间为4h；
步骤4、CdZnTe外延膜的生长：打开近空间升华炉，将经过预处理的多晶源和衬底放入升华炉，开启机械泵和通气阀，待腔体真空度低于5Pa时分子泵自动接入，将腔内真空度抽至0.05Pa，运行步骤3的生长程序并打开水冷，待程序运行完成且炉内冷却至室温，依次关闭通气阀、分子泵及水冷，取出CdZnTe/GaAs外延膜；
步骤5、CdZnTe外延膜的退火：打开近空间升华炉，将退火源和CdZnTe/GaAs外延膜放入升华炉，开启机械泵和通气阀，待腔体真空度低于10Pa时运行退火程序；退火为恒温退火，退火源为粉状Te单质；上下加热台分别控制CdZnTe/GaAs外延膜与退火源的温度；打开水冷并关闭通气阀和机械泵，待程序运行完成且炉内冷却至室温，关闭水冷，制备完成CdZnTe/GaAs外延膜。
3.根据权利要求2所述的方法，其特征在于：所述超声清洗为20～25分钟。
4.根据权利要求2所述的方法，其特征在于：所述GaAs衬底的面积小于多晶源的面积。
5.根据权利要求2所述的方法，其特征在于：所述粉状Te单质纯度为7N。
6.一种采用权利要求1所述CdZnTe/GaAs外延膜的CdZnTe探测器，其特征在于：在CdZnTe/GaAs的外延膜和衬底表面上，结合不超过100nm的金电极层，形成Au/CdZnTe/p-GaAs/Au探测器。
7.一种采用权利要求1所述CdZnTe/GaAs外延膜的CdZnTe探测器，其特征在于：采用真空蒸镀法，将CdZnTe/GaAs外延膜放入蒸镀机，将真空度抽至0.005Pa，分别在外延膜和衬底表面蒸镀80nm的金电极层，形成Au/CdZnTe/p-GaAs/Au探测器。
8.一种权利要求6或7所述CdZnTe探测器的应用方法，其特征在于：所述Au/CdZnTe/p-GaAs/Au探测器用于对241Am@59.5KeVγ射线的响应。
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